气相色谱法测定富马酸卢帕他定原料中的残留溶剂

GC determination of residual solvents in fumarate rupatadine

目的:用毛细管柱气相色谱法建立残留溶剂(正己烷、四氢呋喃、乙睛、氯仿、甲苯)的测定方法。方法:采用 EC^(TM)-Wax(30 m×0.53 mm×1.20μm)毛细管柱,以氮气为载气,FID 检测器,采用程序升温,柱温为60℃,保持5 min,以40℃·min^(-1)的速度升到140℃,保持5 min,进样口温度250℃,分流直接进样,外标法计算残留溶剂的含量。结果:在考察的浓度范围内呈现良好的线性关系(正己烷 r=0.9990、四氢呋喃 r=0.9996、乙腈 r=0.9991、氯仿 r=0.9992、甲苯 r=0.9997),平均回收率范围为97.8%～102.0%,理论塔版数均大于9000,相邻的峰的分离度均大于2,精密度、重复性 RSD 均小于4.0%。结论:本方法简单、结果准确、重现性好,可用于富马酸卢帕他定中正己烷、四氢呋喃、乙腈、氯仿、甲苯5种残留溶剂的同时测定。

Objective：To establish a method for determining the residues of kinds of solvents by capillary gas chro-matography. Method：The capillary was ECTM-Wax （30 m×0.53 mm×1.20 μm）. The carrier gas was nitrogen gas and FID was as detector. The injector temperature was 250℃ and the detector temperature was 250 ℃. The column temperature program was initial temperature 60 ℃（hold 5 min） ,with the increase rate of 40 ℃·min^-1 to 140℃ （ hold 5 min）. The assay of residual solvents were calculated by external standard method. Results： It appeared a good linearity in the experimental concentration （r = 0. 9990 -0. 9997 ）. The rate of recovery has the rang of 97.8% - 102. 0%. The number of theoretical plates were more than 9000 and the resolutions between the adjacent peaks were more than 2. The RSD of precision and accuracy were all less than 4%. Conclusion：The method is simple, sensitive accurate, and can be used for detection of five residual solvent in fumarate rupatadine.